IBP1034_12 A NOVEL VISCOELASTIC SURFACTANT SUITABLE FOR USE IN HIGH TEMPERATURE CARBONATE RESERVOIRS FOR DIVERTED ACIDIZING STIMULATION

TREATMENTS Stuart Holt1, Jian Zhou2, Fred Gadberry3, Hisham Nasr-El-Din4 and Guanqun Wang5
Copyright 2012, Brazilian Petroleum, Gas and Biofuels Institute - IBP
This Technical Paper was prepared for presentation at the Rio Oil & Gas Expo and Conference 2012, held between September, 1720, 2012, in Rio de Janeiro. This Technical Paper was selected for presentation by the Technical Committee of the event according to the information contained in the final paper submitted by the author(s). The organizers are not supposed to translate or correct the submitted papers. The material as it is presented, does not necessarily represent Brazilian Petroleum, Gas and Biofuels Institute opinion, or that of its Members or Representatives. Authors consent to the publication of this Technical Paper in the Rio Oil & Gas Expo and Conference 2012 Proceedings.

Abstract
Due to the low permeability of many carbonate hydrocarbon-bearing reservoirs, it is difficult to achieve economic hydrocarbon recovery from a well without secondary stimulation. Bullheading of strong acids, such as HCl is practiced in low temperature reservoirs, but as the bottom hole temperature (BHT) rises, the acid becomes increasingly corrosive, causing facial dissolution and sub-optimal wormhole network development. In the last decade, viscoelastic surfactants (VES) have been added to HCl acid systems to improve the stimulation of HT carbonate reservoirs. The VES form living polymers or worm-like micelles as electrolyte concentration rises in the acid due to reaction with the reservoir. This leads to viscosification of the stimulation fluid. The viscosification slows further acid reaction in the region already contacted by the acid, and forces the acid to take an alternate path into the rock, leading to diversion of the acids further down the well to the harder to access toe or lower permeability zones. Until recently, the maximum BHT that such VES-based diverting systems could be used was up to about 250F/120C. Above that temperature, all viscous properties of the fluid are lost, destroying the mechanism of acid diversion. A recently developed novel viscoelastic surfactant provides nearly 100F/55C extension in the BHT range in which diverted acid treatments can be used. These fluids are able to maintain both viscosity up to about 375F/190C, with the elastic modulus predominating up to 350F/175C. It is the elasticity which is particularly important in acid diversion. These fluids can have their viscosity readily broken by in-situ hydrocarbons, dilution with water or by using a mutual solvent. The broken fluids are readily removed from the near-wellbore, leaving the newly created wormhole network to produce the target hydrocarbons. The new VES is significantly more environmentally benign compared with current VES technologies.

1. Introduction
To remove or bypass formation damage around the near-wellbore area, an acid-stimulation treatment is one of the most popular methods. Uniform distribution of the treatment fluids over the entire production (or injection) interval is a key factor to determine if the matrix treatment is successful or not. Two main branches of methods to improve acid distribution have been described (Hill and Rossen 1994): mechanical (mechanical zone isolation (packers), ball sealers, coiled tubing), and chemical (foam, particulate diverting agents, and viscosified acids). Mechanical techniques have proved to be more expensive and time consuming than chemical techniques (Nasr-ElDin et al. 2007). Another disadvantage is that they are often neither applicable nor effective in openhole wells. Solid bridging materials are good candidates, but they can bring operational difficulties and have the potential to cause plugging of the near-wellbore if over-treated (Economides and Nolte 2000). Acid placement methods should meet the

______________________________ 1 Bachelor, Global Innovation Manager Oilfield AkzoNobel Surface Chemistry 2 Ph.D., Section Head AkzoNobel Surface Chemistry 3 Ph.D., Senior Scientist AkzoNobel Surface Chemistry 4 Professor, Department of Petroleum Engineering - Texas A&M University 5 Ph.D. Student, Department of Petroleum Engineering - Texas A&M University

Rio Oil & Gas Expo and Conference 2012 following requirements: cause no more formation damage, compatible with formation fluids, easy to be cleaned up, and stable at the downhole conditions. Acid diversion is important during acidizing in vertical wells with long target zone, horizontal and multilateral wells. It is also important when the target zone is heterogeneous with various lithologies (calcite and dolomite) or with significant variation in permeability. Viscoelastic surfactant (VES) can be added to the acid to direct the acid into low permeability or damaged zones. Good diversion requires developing high viscosity and elasticity (Gomaa et al. 2010). The authors stressed on the importance of elasticity in depleted acids to provide acid diversion, particularly where there is permeability contrast, dramatically improving the placement of acid over the wellbore interval. VES have been used in the industry for several stimulation applications as diverting agents to improve the distribution of the acid treatments (Alleman et al. 2003; Zeiler et al. 2006). The characteristics of VES can significantly increase the apparent viscosity of the fluid. The viscosity buildup was accomplished by forming worm-like micelles (Samuel et al. 1997). Therefore, VES can be used to add diverting ability to the fluid in acidizing treatments. VESbased acid systems can be good fracturing fluids (Weaver et al. 2001) and matrix acidizing fluids (Chang et al. 2001a,b; Nasr-El-Din et al. 2003). However, most conventional VESs do not tolerate high temperatures. VES tends to degrade over time with exposure to heating and loses its high viscosity (Huang and Crews 2008a; Yu et al. 2011). The best VES can only provide stable viscosity up to 250oF with the addition of a stabilizer (Crews et al. 2008; Huang and Crews 2008b). VES based acid can be cleaned up easily and provide higher regained permeability than conventional gelled acid systems (Lungwitz et al. 2007). It is believed that VES can be dissolved in hydrocarbons so that no cleanup treatment is needed after flushing VES-based fluid. However, at least 80% of the injected surfactant is retained inside the core (Yu et al. 2010). When reservoir or injection fluid does not naturally break the VES in-situ gel, post-flush of mutual solvent and/or adding an internal breaker at the beginning is recommended to ensure the breaking of the gel (Samuel et al. 1999; Jiang 2002; Crews 2005; Nasr-El-Din et al. 2006) and regain permeability. The mutual solvent ethylene glycol monobutyl ether (EGMBE), was first introduced to the oil/gas industry for acid treatments in sandstone reservoirs (Gidley 1971).

2. Experimental Studies
2.1. Materials Hydrochloric acid (ACS reagent grade) was titrated using 1N sodium hydroxide solution to determine its concentration, which was 36.8 wt%. All acid solutions were prepared using deionized (DI) water with a resistivity of 18.2 M.cm at room temperature. The new VES, a zwitterion surfactant, and three commercial corrosion inhibitors (CI) were used without further purification. ACS grade CaCl2 was used to prepare spent VES-based acid solutions. A 100% pure hexane was used to break VES gels. A cylindrical core plug was cut from an Indiana limestone block with an initial permeability of 140 md. The core was cut with a length of 20-in and 1.5-in diameter. 2.2. Preparation of Live Acids When preparing 100 g of live VES-based acid, 40 g of DI water was first weighed in a beaker. Then 1 cm3 corrosion inhibitor was added. A magnetic stirrer was used to mix the solution. After 5 minutes, 55 g of 36.8 wt% HCl was added to the solution slowly. After another 10 minutes, 4 cm3 of new VES was slowly added to the acid. Then the acid solution was mixed for 30 minutes before injection. 2.3. Preparation of Spent Acids Most of the experiments in this paper were performed using 30 wt% CaCl2 and 6 vol% viscoelastic surfactant. A blender was used to mix these solutions. The whole mixture was blended well at a high shear rate for 3 min. A considerable number of air bubbles remained in the formulations after mixing. These bubbles were removed by centrifuging for 15 minutes at 1250 rpm. 2.4. Rheology Measurements A fresh sample of spent VES-based acid was prepared, and nearly 52 cm3 of the sample was loaded into the sample cup of the rheometer to measure its viscosity. The Grace Instrument M5600 HPHT Rheometer was used to measure the apparent viscosity of surfactant formulations under different conditions. The wetted material is Hastelloy C-276, which is corrosion resistant. The rheometer can measure viscosity at various temperatures up to 500F, over shear rate of 0.00004 to 1,870 s-1. The elastic modulus (G) and viscous modulus (G) can be examined over frequency of 0.01 to 5 Hz. A B5 bob was used in this work which requires a sample volume of 52 cm 3. A pressure of 400 psi was applied to minimize evaporation of the sample, especially at high temperatures. 2

Rio Oil & Gas Expo and Conference 2012 2.5. Core Preparation 1. A limestone core was dried at 100C for 3 hours and weighed to obtain its dry weight; then it was saturated with DI water under vacuum for 24 hours and the wet weight was measured. The core porosity was 16% and the pore volume was nearly 93.5 cm3. 2. The DI water saturated core was scanned using CT before acid injection, and the CT number was found to be 1,700-1,800. 3. The core was placed inside the core holder, Fig. 1. Water was injected at different rates and the corresponding pressure drops were obtained to calculate the initial permeability of the core. 4. VES-based acid was injected at 5 cm3/min, while the pressure drop across the core was monitored and recorded. The injection of acid was stopped when breakthrough occurred, and then switched to DI water with the same rate until the pressure drop was stabilized. 5. The core was examined by CT scan to observe the wormholes generated by the acid. The core was water saturated during the scan.

Fig. 1: Coreflood Setup.

3. Results and Discussion

3.1. Ecotoxicity Testing The ecotoxicological impact of this technology on the environment was evaluated by a series of studies conducted on the new VES. Biodegradation and toxicity to marine and freshwater organisms were tested under standard conditions to GLP standard, unless stated. Results for these tests were extremely favorable, with EC/LC50 concentrations in excess of 100mg/l for a variety of organisms playing different of roles in aqueous ecosystems. The surfactant is also readily biodegradable in freshwater, indicating the substance will not persist in the environment if released. Advanced multi-software modeling predicts the material to have a low degree of toxicity to mammals. Together this data represents significant ecotoxicological improvement over other viscoelastic surfactant types that can also be used in this area, such as amine oxides and quaternary ammonium salts. Biodegradation was tested with the method: OECD (1992) Guideline for testing of chemicals, Degradation and accumulation, No. 301: Ready biodegradability, Paris Cedex, France. The total test period was 28 days. With 61% of the chemical degrading in this period, the substance is considered readily biodegradable. Acute Toxicity to freshwater carp (Cyprinus carpio) was tested with the method: EPA Ecological Effects Test Guidelines, OPPTS 850.1075, Fish Acute Toxicity Test, Freshwater and marine also compliant with EPA 712-C-96-118 April 1996. The concentration of the chemical was 100 mg/L with a test period of 96 hours. The 96hr-LC50 was >100 mg/L. The nominal concentration was 100 mg/L with a measured concentration of 14mg/L. No observed effect concentration was 14 mg/L. Acute Toxicity to freshwater water flea (Daphnia magna) was measured with the method: OECD, 2004. Daphnia sp., acute immobilization test. Guidelines for testing of chemicals nr. 202, 13 April 2004. Organization for Economic Co3

Rio Oil & Gas Expo and Conference 2012 operation and Development, Paris. The concentration of the chemical was 100 mg/L with test period of 48 hours. LC50 was >100 mg/L and the no observed effect concentration = 100 mg/L. Acute toxicity to brine shrimp (Artemia salina) was conducted with the test method: OECD, 2004. Daphnia sp., acute immobilization test, replacing organism with Artemia Salina. Guidelines for testing of chemicals nr. 202, 13 April 2004. Organization for Economic Co-operation and Development, Paris. The concentration of the chemical was 100 mg/L with a test period of 48 hours. LC50 was >100 mg/L and the no observed effect concentration = 100 mg/L. Acute toxicity to freshwater green algae (P. Subcapitata) was tested with the method: OPPTS 850.5400 Algal Toxicity Tiers I and II EPA April 1996, and OECD, 2006. Freshwater alga and cyanobacteria, Growth Inhibition Test, Test Guideline 201, March 23rd, 2006. The concentration of the chemical was 100 mg/L with test period of 72 hours. ErC50 (72h) was >1048.5 mg/L with the no observed effect concentration (NOEC) of 327 mg/L. Meanwhile, the lowest observed effect concentration (LOEC) was >1,048.5 mg/L. Acute toxicity to marine algae (P. Tricornutum) non-GLP was tested with the method: OPPTS 850.5400 Algal Toxicity Tiers I and II EPA April 1996, and OECD, 2006. Freshwater alga and cyanobacteria, Growth Inhibition Test, Test Guideline 201, March 23rd, 2006. Adapted for P. Tricornutum. The concentration of the chemical was 100 mg/L with test period of 72 hours. ErC50 (72h) was >1048.5 mg/L with the no observed effect concentration (NOEC) of 102 mg/L. Meanwhile, the lowest observed effect concentration (LOEC) was greater than 327 mg/L. 3.2. Rheology Measurements Fig. 2 shows the apparent viscosity as a function of time at 350F and shear rate of 100 s -1 for the solution containing 6 vol% viscoelastic surfactant in a 30wt% CaCl 2 brine. It can be seen that the viscosity increased with the temperature at the beginning until 250F, and then decreased with higher temperatures. Even after one and a half hours heating at 350F, the viscosity still maintained above 100 cp.

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Fig. 2: Apparent viscosity of a 6 vol% surfactant solution in 30 wt% CaCl2 at 350F and 100 s-1.

Temperature (oF)

Rio Oil & Gas Expo and Conference 2012 The elastic modulus (G) and viscous modulus (G) were measured at frequency of 1 Hz and 400 psi for 6 vol% surfactant formulation. Fig. 3 shows that the system was not very elastic or viscous when the temperature was low, but at higher temperatures >170F, the elastic modulus increased dramatically. Two cross-over temperatures were observed and good capability to carry the sand and proppant can be expected between 180 and 350F.

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Fig. 3: G and G of solution containing 6 vol% surfactant and 30 wt% CaCl2 It is known that hydrocarbons can break wormlike micelles (Fu and Chang, 2005). Fig. 4 shows that apparent viscosity of the surfactant in brine system decreased with the addition of hexane. More concentrated hexane was used, lower viscosity was obtained. The results indicate that the surfactant system can tolerate the hexane contamination up to 0.5% without significant reduced performance. (Wang et al, 2012) .

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Fig. 4: Effect of hexane on the apparent viscosity of solution containing 6 vol% surfactant and 30 wt% CaCl2. 3.4. Coreflood Study A coreflood on a carbonate core (20 in.) was conducted at 325F, at which the spent VES-based acid had the highest viscosity. Indiana limestone with an initial permeability of 140 md was used. DI water was injected first, and when the pressure drop across the core stabilized at 325 F, the new VES-based 20 wt% HCl with 1 vol% corrosion inhibitor was injected at 5 cm3/min until breakthrough. The pressure drop across the core was recorded as shown in Fig. 5. DI water was injected at the beginning and when pressure drop stabilized, the VES-based acid was injected. Pressure drop started to increase because of the higher viscosity of VES-based acid than water. Then, when a wormhole was created, pressure drop started to decrease. With increased concentration of calcium cations and pH value of the fluid, wormlike micelles started to form, and significantly increased the fluid viscosity. An increase in the pressure drop was observed. Next, the acid created another wormhole and tried to pass through the whole core. Thus, we observed a decrease of pressure drop again. Similar processes were repeated until we switched the injection fluid to DI water. After taking the core from the core holder, a photo of the inlet was taken (Fig. 6) and multiple wormholes were noted at the inlet face of the core. However, only one dominant wormhole was observed on the outlet face of the core (Fig. 7). After the whole system cooled down to room temperature, final permeability of the core was measured with DI water at various injection rates and it was nearly 1091 md.

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Fig. 5: Pressure drop across the core during the coreflood test.

Wormhole Wormhole

Fig. 6: Inlet face of the 20-inch Indiana Limestone core after test with 4 vol% VES-based 20 wt% HCl.

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Wormhole

Fig. 7: Outlet face of the 20-inch Indiana Limestone core after test with 4 vol% VES-based 20 wt% HCl.

Fig .8: CT scan images of the core after treatment. 8

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3.5. CT Scan The core was CT scanned after treatment to observe the propagation of the wormhole (Fig. 8). Multiple wormholes were created near the inlet, and one dominant wormhole was observed close to the outlet. There were not only multiple wormholes, but we also observed that the dominant wormhole kept changing its direction through the core. The diameter of the wormhole decreased from the inlet to the outlet of the core. Since only one third pore volume of VES-based acid was injected, no breakthrough was observed and the length of the wormhole was nearly 16 in.

4. Conclusions
A new VES-based system was developed to extend the range of applicable temperatures. Rheology measurements were conducted up to 350 F. A coreflood study was conducted to evaluate the performance of the new VES-based acid at reservoir conditions, and to observe the propagation of wormholes in a limestone core. Based on the results obtained, the following conclusions can be drawn: 1. 2. The new VES-based fluid exhibited higher viscosity at elevated temperatures. It reached its peak around 250F and still can maintain its viscosity above 100 cP at 100s-1 up to 350F. When the fluid temperature was between 180 and 350F, the fluid is elastic modulus dominant, which indicates that the acid will be effectively diverted as it applied, leading to optimized wormhole networks in either conventional or fractured carbonate reservoirs. Addition of a model hydrocarbon (hexane - an analogue for crude oil) or a mutual solvent (EGMBE) to the gelled depleted acid significantly decreased the viscosity of the fluid and can act as in-situ and/or post-addition breakers respectively. The VES-based acid changed its propagation direction during the core flood test, and multiple wormholes were created at the inlet face of the core at 325F. Limited face dissolution was observed. The new VES exhibits significant improvement in environmental characteristics when compared with other VES systems commonly used today.

3.

4. 5.

This new fluid provides a viable solution for ultra-high temperature mineral acid stimulation of carbonate reservoirs.

5. Acknowledgements
The authors would like to thank AkzoNobel Surface Chemistry for their financial support for this work and the collaboration received from Texas A&M University in developing this technology.

6. References
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